Regueiro Jorge, Llompart Maria, Psillakis Elefteria, Garcia-Monteagudo Juan C, Garcia-Jares Carmen
Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Santiago de Compostela, Santiago de Compostela, Spain.
Talanta. 2009 Oct 15;79(5):1387-97. doi: 10.1016/j.talanta.2009.06.015. Epub 2009 Jun 12.
Simultaneous ultrasound-assisted emulsification-microextraction (USAEME) and derivatization combined with gas chromatography-tandem mass spectrometry (GC-MS/MS) is proposed for the first time for the analysis of parabens, triclosan and related phenols in water samples. In situ acetylation was successfully applied for the derivatization of target compounds with high efficiency using non-expensive reagents. The proposed method exhibits many advantages such as simplicity, efficiency, low cost, and minimum solvent consumption. In addition, the whole analytical process, including sample preparation and determination, is performed in only 20 min. A multifactorial experimental design was employed to study and optimize the main variables potentially affecting the microextraction and derivatization processes (extraction solvent, phase ratio, sodium chloride concentration, extraction time, and acetic anhydride volume). The performance of the method was studied in terms of accuracy, linearity, precision, and enrichment factor. Quantitative recoveries (>or=85%) were obtained for all target compounds, and method precision was also satisfactory (RSD<or=13%) even for complex samples. Enrichment factors ranging from 100 to 200 were obtained, allowing achieving limits of detection at the low picogram per millilitre for most of the target compounds. Several real samples, including wastewaters, river waters and swimming pool water, were analyzed. Since matrix effects were not observed, quantification can easily be performed using external calibration with acetylated standards, allowing a high sample throughput.
首次提出将同步超声辅助乳化微萃取（USAEME）与衍生化相结合，并与气相色谱 - 串联质谱（GC - MS/MS）联用，用于分析水样中的对羟基苯甲酸酯、三氯生及相关酚类。使用非昂贵试剂成功实现了原位乙酰化，高效地对目标化合物进行衍生化。该方法具有诸多优点，如操作简单、效率高、成本低且溶剂消耗最少。此外，整个分析过程，包括样品制备和测定，仅需20分钟即可完成。采用多因素实验设计来研究和优化可能影响微萃取和衍生化过程的主要变量（萃取溶剂、相比、氯化钠浓度、萃取时间和乙酸酐体积）。从准确度、线性、精密度和富集因子方面对该方法的性能进行了研究。所有目标化合物的定量回收率均大于或等于85%，即使对于复杂样品，方法精密度也令人满意（相对标准偏差小于或等于13%）。获得了100至200的富集因子，使得大多数目标化合物的检测限低至每毫升几皮克。分析了包括废水、河水和游泳池水在内的多个实际样品。由于未观察到基质效应，使用乙酰化标准品进行外标法校准即可轻松实现定量，从而实现高样品通量。
